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Sensory descriptive analysis of aged feng-flavored Baijiu liquor indicated notable differences in samples of different ages. The samples of freshly distilled Baijiu and those with shorter storage times exhibit bran and fresh green flavors, whereas, with increasing storage time, honey, sweet, and floral fragrances are gradually enhanced. Samples of feng-flavored Baijiu were prepared using headspace solid-phase microextraction, followed by comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry. A total of 496 compounds were identified in all samples, mainly categorized as 14 groups of substances, including esters and aldehydes. Interestingly, 42 of these substances were found in Feng-flavored Baijiu for the first time. Chemometrics was used to analyze the key differential compounds. First, 143 differential compounds closely related to aging were preliminarily screened, and principal component analysis revealed that these compounds were separated by baijiu age. Then, 65 differential compounds were selected by partial least squares discriminant analysis. Furthermore, 43 key differential compounds were selected by combined analysis with variable importance in projection and Pearson correlation coefficients. Partial least squares regression was used to study the correlation between the sensory properties and key differential compounds, and the results indicated that most compounds were closely related to the aging period of the Baijiu. The results of this study provide a theoretical basis and reference for flavor research on feng-flavored Baijiu. Full article